Manufacture of artificial silk



Patented Jan. 5, 1937 UNITED STATES PATENT OFFICE MANUFACTURE or ARTIFICIAL smn Louis Barthelemy, Rome, Ga., assignor to Tubiz'e Chatillon Corporation, New York, N. Y., a; corporation of Delaware No Drawing. Application August 13, 1935,

Serial No. 35,973

4 Claims. (e1; 106-40) 1 'I'hisinvention relates to the production of artificial silk of improved hand and subdued lustre, and contemplates an improved artificial silk of this character, and a novel spinning solu tion from which such artificial silk may be produced. More specifically, the invention is concerned with the incorporation of insoluble alcohols into spinning solutions and into artificial silk filaments produced from these spinning solulO tions.

As a result of my investigations, I have discovered that artificial silk filaments having a subdued lustre and of excellent hand and suppleness may be produced by incorporating thereinto insoluble alcohols derived from or constituents of fats and waxes, such as cetyl alcohol, stearyl alcohol, oleyl alcohol, cholesterol, carnaubyl alcohol, or ceryl alcohoL. When insoluble alcohols of this character are incorporated into a spinning solution, artificial silk filaments produced I from such solutions are exceedingly supple, have a downy touch, and are suitable for immediate fabrication withoutadditional treatment.

Based on this discovery the present invention involves the incorporation and/or dispersion of insoluble alcohols derived from fatty materials into spinning solutions, and spinning artificial silk filaments therefrom with the result thatartificial silk of subdued lustre, great suppleness and soft hand are produced:

The term insoluble is here used to mean sub stantially insoluble in water. 'By fatty mate-- rials I mean organic fats and waxes.

Among the insoluble alcohols derived from fatty materials which may advantageously be used in the practice ofv the invention are: I

(,1) Alcohols of the ethane series such as cetyl' alcohol, s'tearyl alcohol, ceryl alcohol, carnaubyl alcohol, octodecyl alcohol. (2) Alcohols of unsaturated series such as olefine alcohols and diolefine alcohols; and

(3)' Alcohols of the cyclic series, such as zoosterols (cholesterol, isocholesterol, etc.) and phytosterols (sitosterols, brassicasterols, etc.). Alcohols of this cyclic series may be described convenientlyassterols. 1 a

, The aforementioned insoluble alcohols derived from fatty materials may be incorporated and dispersed in the spinning solution in any suitable manner. They may be warmed if necessary to a temperature above their melting point, and be directly whipped or beaten into the spinning solution by means of a' suitable dispersing device, such as a so-called colloid mill., They may be first mixed with a portion of the spinning solution, and the resulting mixture then added to and mixed with the remainder of the spinning solution. In some cases, it may be convenient to mix the insoluble alcohols with a volatilesolventsuch as acetone or ethyl ether, the result- 5 ing mixture then being incorporated into the spinning solution by mixing.

The insoluble alcohols may also be incorporated into the spinning solution by first mixing them with mineral oil or other oleaginous com- 10 pound with which they are miscible and thereafter incorporating the mixture into the spinning solution. In the event that mineral oils. or other oleaginous materials are mixed with the alcohols prior to incorporation into the spinning 15 solution, it is frequently convenient to add a small amount of stabilizing material, such as sulphonated oil, sulphonated alcohols or related compounds such as stearyl alcohol sodium sulphonate. I v 20 Following thorough agitation in order to insure uniformity of dispersion of the insoluble alcohols in the spinning solution, the solution may be spun in the manner customary for the particular variety of the artificial silk being manu- 25 factured, employing the customary coagulants.

I attribute the subdued lustre, the increased suppleness and the improved hand of artificial silk produced according to my invention to the presence of fine particles of insoluble alcohols 0 dispersed throughout the filaments' Microscopic examination of the filaments leads me to believe that the fine particles of insoluble alcohols are present in the form of talcky flakes. I believe that these flakes act as internal lubricants within 35 the filaments and thus account for the increased suppleness and softer hand. At the same time, the presence of the flakes serves to change the refractive index of the filaments to light and thus produces the subdued lustre. c 40 When insoluble alcohols are used in conjunc- .tion with mineral oil or other oleaginous comthe amount of mineral oil alone. The action of 55 insoluble alcohols impart an increased suppleness and improved hand to artificial silk filaments in which they are incorporated, at the same time accomplishing a marked delustering of the material.

, My invention will be more thoroughly undenstood in the light of the following examples, which illustrate practices of the invention:

Ezamplef Into 1000 parts of. a fresh viscose solution maintained at 18 C. and containing 7% of cellulose, is emulsified partsof a mixture oi:

- 7 Parts Mineral oil of sec. Saybolt viscosity at F 59 Stearyl alcohol 40 Stearyl alcohol-sodium sulfonate .1

The mixture of. mineral oil, stearyl alcohol an stearyl-alcohol sodium sulphonate should be prepared at 50 C. and then cooled rapidly during continuous agitation to 30 C.

The resulting viscose-mineral oil stearyl alcohol emulsion is aged for about sixty hours or until it'attains a 10.4 Hottenroth index of ripeness. The emulsion is then spun into a coagulating bath containing 9.5 parts of sulfuric acid and 200 parts sodium sulfate per 1000 parts of water, and filaments are thus produced.

The lustre of the filaments produced in this manner is not only similar to that of natural silk, but after desulfurization and washing, the yarn is naturally soft with a feather-like feel. No special scour of sizing is necessary to render it suitable for fabrication.

Example H lustre and an increased softness as compared with. a yarn which has'been delustred with mineral oil alone. 1

' Example III To 1000 parts of a fresh viscose solution, maintained at 18 C. and containing 7% of cellulose are added 60 parts of a mixture consisting of equal proportions of a white mineral oil of '75 sec. Saybolt viscosity at 100 F. and stearyl alcohol,

together with 10 parts of finely divided titanium dioxide. The resulting mixture is thoroughly emulsified andthe viscose is spun in a G -m ting bath similar to that used in Example I. The resulting artificial silk filaments are highly delustered, are of superior softness and have a downy The invention may be utilized in the production I of any of the customary varieties of artificial silk. In viscose or cupra-ammonium silks, the insoluble alcohol or alcohols are present in the spinning solution in a finely emulsified condition. In acetonic collodion or cellulose acetate or etheralcohol collodion of nitrocellulose the insoluble alcohol, or a mixture of insoluble alcohols may be in solution. In either case, after spinning the insoluble, alcohols are more or less uniformly dispersed as fine plate-like particles throughout the artificial silk filaments.

The heterogeneous dispersion of the mixture of stearyl alcohol and mineral oil (as in the foregoing examples) gives a particularly pleasing artifiicial silk. The mineral oil employed is preferably white in color, substantially non-acid, having a Saybolt viscosity of from 65 to 100, measured at 100 F.

' It will be understood that the examples given herein are intended to be purely illustrative and not restrictive. Changes in procedure will undoubtedly occur to the manskilled in the art, without, however, departing from the basic concept of my invention.

I claim:

1. An artificial cellulosic silk filament having substantially uniformly dispersed therein mineral oil and flakes of a water insoluble alcohol in such relative proportions that lustre of the filament is reduced and hand and suppieness oi the filament are improved, the insoluble alcohol being selected from the group consisting in cetyl alcohol, stearyl alcohol, ceryl alcohol, carnaubyl al- .cohol, octadecyl alcohol and oleyl alcohol, oiefine alcohols, diolefine alcohols, zoosterols and phvtosterols.

2. An artificial cellulosic-silk filament havin substantially uniformly dispersed therein mineral oil and flakes of stearyl alcohol in such relative proportions that lustre of the filament is reduced and hand and suppleness of the filament are improved.

3. An artificial cellulosic silk filament having substantially uniformly dispersed therein mineral oil and flakes of oleyl alcohol in such relative proportions that lustre of the filamentis reduced and hand and supppleness of the filament are improved.

proved, the insoluble alcohol being selected from the group consisting in cetyl alcohol, stearyl alcohol, ceryl alcohol, carnaubyl alcohol, octodecyl alcohol'and oleyl alcohol, olefine alcohols, diolefine alcohols, zoosterols and phytosterols.

HENRI LOUIS BAR'I'HEIEMY. 

